O-Phenylenediamine → 6-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid (2-amino-phenyl)amide

HRID 12282ノート

反応式

HRID 12282 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([OH:11])=O)[C:5](=[O:8])[NH:6][N:7]=1.[C:12]1([NH2:19])[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[NH2:18].Cl.C(N=C=NCCCN(C)C)C>CN(C1C=CN=CC=1)C.CN(C=O)C>[NH2:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[NH:19][C:9]([C:4]1[C:5](=[O:8])[NH:6][N:7]=[C:2]([Cl:1])[CH:3]=1)=[O:11]

参加物

6

反応物 3

HCID 7243O-PhenylenediamineHCID 3340156-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 866116096-Chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid (2-amino-phenyl)amide

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

30.5 g of 6-chloro-3-oxo-2,3-dihydropyridazine-4-carboxylic acid, 18 g of ortho-phenylenediamine and 2 g of DMAP are dissolved in 800 ml of DMF, at room temperature 32.2 g of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride are added, and the resulting solution is stirred at room temperature for 4 hours. For workup, the solvent is distilled off and the residue is suspended in water at 70° C. The precipitate is filtered off, washed several times with water and then dried in vacuo.

後処理

  1. additionare added
  2. distillationFor workup, the solvent is distilled off
  3. customis suspended in water at 70° C
  4. filtrationThe precipitate is filtered off
  5. washwashed several times with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-9feb74f319eb4940b9784589c395aa8d
出典データセット
uspto-grants-2010_06
特許番号
US07727989B2

反応ノート

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